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Measurement of trace components using D/teX Ultra

Background

The MiniFlex can be equipped with the D/teX Ultra high-speed 1-dimensional detector to obtain greater intensity. By using this detector, it is possible to obtain intensity a few tens to roughly 100 times greater than a scintillation counter. Using this feature, it is possible to greatly reduce measurement time, detect trace components, and measure micro-samples with high sensitivity.

Investigation

Fig. 1 shows the diffraction profiles obtained with a scintillation counter and the D/teX Ultra high-speed 1-dimensional detector. The D/teX Ultra detector measures data faster because it can measure a wide range of 2θ simultaneously with good angular resolution.

Diffraction profiles when using a scintillation counter and high-speed 1-dimensional detector
Figure 1: Diffraction profiles when using a scintillation counter and high-speed 1-dimensional detector

Fig. 2 shows the results of quantifying an extreme trace amount of anatase contained in a rutile reagent using the standard addition method (measurement time 1 minute for 1 sample). As a result of measurement, it was found that the rutile reagent contains about 0.14 mass% of anatase. In this way, using the D/teX Ultra high-speed 1-dimensional detector enables evaluation with good sensitivity and a short measurement time of trace components contained at a rate of 1 mass% or less. 

X-ray diffraction pattern and quantitative analysis results for trace anatase contained in rutile reagent
Figure 2: X-ray diffraction pattern and quantitative analysis results for trace anatase contained in rutile reagent

Apparatus condition:

MiniFlex600 (F.F tube 40 kV, 15 mA), Detector: D/teX Ultra, Slit conditions: DS = 1.25°, SS = 8 mm, RS = 13mm, Incident side and receiving side Soller slit: 5°, Incident height limiting slit = 10 mm

Measurement condition:

Scan range: 2θ = 24.9 ~ 25.6°, Step width: 0.02°, Scan speed: 1° / min. (about 1 min.)